# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_footnote _publ_author_address K.Baranowska . ; Department of Inorganic Chemistry, Faculty of Chemistry, Gda\'nsk University of Technology 11/12 G. Narutowicz St., 80233 - PL Gda\'nsk, Poland ; R.Grubba . ; Department of Inorganic Chemistry, Faculty of Chemistry, Gda\'nsk University of Technology 11/12 G. Narutowicz St., 80233 - PL Gda\'nsk, Poland ; E.Matern . ; Institut f\"ur Anorganische Chemie, Universit\"at Karlsruhe (TH), D-76128 Karlsruhe ; J.Pikies . ; Department of Inorganic Chemistry, Faculty of Chemistry, Gda\'nsk University of Technology 11/12 G. Narutowicz St., 80233 - PL Gda\'nsk, Poland ; A.Wisniewska . ; Department of Inorganic Chemistry, Faculty of Chemistry, Gda\'nsk University of Technology 11/12 G. Narutowicz St., 80233 - PL Gda\'nsk, Poland ; _publ_contact_author_address ; Department of Chemistry Gda\'nsk University of Technology Narutowicza 11/12, PL-80233 Gda\'nsk, Poland ; _publ_contact_author_email pikies@chem.pg.gda.pl _publ_contact_author_fax '048 58 3472694' _publ_contact_author_phone '048 58 3472351' #----------------------------------------------------------------------------# # SUBMISSION DETAILS # #----------------------------------------------------------------------------# _publ_contact_author_name 'Pikies, Jerzy' _publ_requested_coeditor_name ? #----------------------------------------------------------------------------# # TITLE AND AUTHOR LIST # #----------------------------------------------------------------------------# _publ_section_title ; Reactions of (R~2~N)~2~P--P(SiMe~3~)Li (R = ^i^Pr and Et)with Cp~2~MCl~2~(M = Zr, Hf) and with CpZrCl~3~. Syntheses and Structures of the firstTerminal Phosphanylphosphide Complex of Hafnium [Cp~2~Hf(Cl){\h^1^-(Me~3~Si)P--P(NEt~2~)~2~}]and the first Zirconocene-Phosphanylphosphinidene Dimer [Cp~2~Zr{\m~2~-P--P(NEt~2~)~2~}~2~ZrCp~2~]. ; # END of CIF # Attachment '- ola1k_doCCDC.cif' data_raf3 _database_code_depnum_ccdc_archive 'CCDC 233006' #TrackingRef '- raf3_final.cif' _audit_creation_date 2010-07-28 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ; FM 2010-07-28 # Formatted by publCIF ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Bis[\m-{bi(diethylamino)phosphinephosphinideno}-bis-cyclopentadienylo zirconium(IV)] ; _chemical_formula_moiety 'C36 H60 N4 P4 Zr2' _chemical_formula_sum 'C36 H60 N4 P4 Zr2' _chemical_formula_weight 855.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.309(2) _cell_length_b 12.521(3) _cell_length_c 19.225(6) _cell_angle_alpha 90 _cell_angle_beta 105.17(3) _cell_angle_gamma 90 _cell_volume 1930.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 11.2 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KUMA KM4, serial detector' _diffrn_measurement_method \w--2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 1.54 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_unetI/netI 0.1242 _diffrn_reflns_number 3917 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.05 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 3801 _reflns_number_gt 2231 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'KM4 System (Ga\/ldecki, 1996)' _computing_cell_refinement 'KM4 System (Ga\/ldecki, 1996)' _computing_data_reduction 'DATAPROC (Ga\/ldecki, 1996)' _computing_structure_solution 'SHELXS - 97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia,1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+2.2757P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3801 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.074 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.185 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.47702(9) 0.00974(5) 0.40203(4) 0.0169(2) Uani 1 1 d . . . P1 P 0.6533(3) 0.10900(15) 0.51508(11) 0.0194(4) Uani 1 1 d . . . P2 P 0.6242(2) 0.28337(15) 0.52677(11) 0.0186(4) Uani 1 1 d . . . N1 N 0.7621(8) 0.3020(5) 0.6082(3) 0.0226(14) Uani 1 1 d . . . N2 N 0.7063(8) 0.3311(5) 0.4606(4) 0.0218(14) Uani 1 1 d . . . C1 C 0.9353(10) 0.2655(7) 0.6242(5) 0.0261(18) Uani 1 1 d . . . H1A H 1.0072 0.3262 0.6185 0.031 Uiso 1 1 calc R . . H1B H 0.9447 0.2099 0.5888 0.031 Uiso 1 1 calc R . . C2 C 0.9977(11) 0.2207(7) 0.6993(5) 0.032(2) Uani 1 1 d . . . H2A H 1.0105 0.2787 0.7345 0.048 Uiso 1 1 calc R . . H2B H 1.1056 0.1858 0.7042 0.048 Uiso 1 1 calc R . . H2C H 0.9173 0.1684 0.708 0.048 Uiso 1 1 calc R . . C3 C 0.7282(11) 0.3852(7) 0.6548(5) 0.0285(19) Uani 1 1 d . . . H3A H 0.762 0.359 0.7051 0.034 Uiso 1 1 calc R . . H3B H 0.6062 0.3974 0.6423 0.034 Uiso 1 1 calc R . . C4 C 0.8142(11) 0.4930(7) 0.6517(5) 0.035(2) Uani 1 1 d . . . H4A H 0.9351 0.4824 0.6628 0.053 Uiso 1 1 calc R . . H4B H 0.7883 0.5419 0.6871 0.053 Uiso 1 1 calc R . . H4C H 0.7741 0.5236 0.6034 0.053 Uiso 1 1 calc R . . C5 C 0.8513(10) 0.2906(6) 0.4396(4) 0.0237(17) Uani 1 1 d . . . H5A H 0.8767 0.2179 0.4596 0.028 Uiso 1 1 calc R . . H5B H 0.9483 0.3366 0.4614 0.028 Uiso 1 1 calc R . . C6 C 0.8292(11) 0.2865(7) 0.3600(5) 0.031(2) Uani 1 1 d . . . H6A H 0.7269 0.2472 0.3373 0.046 Uiso 1 1 calc R . . H6B H 0.925 0.2503 0.3498 0.046 Uiso 1 1 calc R . . H6C H 0.8212 0.3593 0.3407 0.046 Uiso 1 1 calc R . . C7 C 0.6427(10) 0.4353(6) 0.4284(4) 0.0224(17) Uani 1 1 d . . . H7A H 0.5487 0.4569 0.448 0.027 Uiso 1 1 calc R . . H7B H 0.5978 0.4253 0.3758 0.027 Uiso 1 1 calc R . . C8 C 0.7663(12) 0.5248(7) 0.4405(6) 0.038(2) Uani 1 1 d . . . H8A H 0.826 0.528 0.4917 0.057 Uiso 1 1 calc R . . H8B H 0.7077 0.5924 0.426 0.057 Uiso 1 1 calc R . . H8C H 0.8461 0.5126 0.4117 0.057 Uiso 1 1 calc R . . C9 C 0.5789(12) -0.0666(8) 0.2992(5) 0.039(2) Uani 1 1 d . . . H9 H 0.5235 -0.0474 0.2511 0.047 Uiso 1 1 d R . . C10 C 0.5383(12) -0.1548(7) 0.3366(5) 0.037(2) Uani 1 1 d . . . H10 H 0.4484 -0.2032 0.3199 0.044 Uiso 1 1 d R . . C11 C 0.6554(12) -0.1572(7) 0.4025(5) 0.032(2) Uani 1 1 d . . . H11 H 0.6611 -0.2096 0.4387 0.038 Uiso 1 1 d R . . C12 C 0.7623(11) -0.0721(7) 0.4075(5) 0.0284(19) Uani 1 1 d . . . H12 H 0.8542 -0.0565 0.4474 0.034 Uiso 1 1 d R . . C13 C 0.7124(10) -0.0118(7) 0.3435(5) 0.0317(19) Uani 1 1 d . . . H13 H 0.7604 0.053 0.3328 0.038 Uiso 1 1 d R . . C14 C 0.3665(11) 0.1955(7) 0.3626(5) 0.034(2) Uani 1 1 d . . . H14 H 0.4369 0.2548 0.38 0.041 Uiso 1 1 d R . . C15 C 0.2520(12) 0.1511(8) 0.3952(5) 0.041(3) Uani 1 1 d . . . H15 H 0.2295 0.1751 0.4386 0.049 Uiso 1 1 d R . . C16 C 0.1760(11) 0.0656(7) 0.3537(5) 0.035(2) Uani 1 1 d . . . H16 H 0.0925 0.0207 0.3635 0.042 Uiso 1 1 d R . . C17 C 0.2424(11) 0.0574(7) 0.2961(5) 0.035(2) Uani 1 1 d . . . H17 H 0.2137 0.0054 0.2589 0.042 Uiso 1 1 d R . . C18 C 0.3607(12) 0.1392(7) 0.3012(5) 0.039(2) Uani 1 1 d . . . H18 H 0.425 0.1529 0.2679 0.047 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0176(3) 0.0170(4) 0.0158(3) 0.0003(3) 0.0040(2) -0.0002(3) P1 0.0195(10) 0.0157(9) 0.0228(11) 0.0001(8) 0.0054(8) -0.0014(8) P2 0.0185(10) 0.0159(9) 0.0220(10) -0.0003(8) 0.0065(8) -0.0010(8) N1 0.020(3) 0.023(3) 0.024(4) -0.007(3) 0.006(3) -0.003(3) N2 0.020(3) 0.018(3) 0.030(4) 0.005(3) 0.010(3) 0.001(3) C1 0.016(4) 0.025(4) 0.036(5) -0.002(4) 0.006(4) -0.001(3) C2 0.031(5) 0.030(5) 0.036(5) -0.006(4) 0.012(4) -0.001(4) C3 0.027(4) 0.030(4) 0.028(5) -0.005(4) 0.007(4) 0.004(4) C4 0.038(5) 0.027(5) 0.040(5) -0.011(4) 0.009(4) -0.004(4) C5 0.022(4) 0.021(4) 0.031(5) 0.011(3) 0.015(4) 0.005(3) C6 0.027(5) 0.034(5) 0.034(5) 0.004(4) 0.013(4) 0.004(4) C7 0.022(4) 0.020(4) 0.022(4) 0.005(3) 0.001(3) 0.009(3) C8 0.041(5) 0.022(4) 0.054(6) 0.003(4) 0.019(5) -0.006(4) C9 0.036(5) 0.057(6) 0.029(5) -0.004(5) 0.016(4) 0.015(5) C10 0.035(5) 0.037(5) 0.044(6) -0.024(5) 0.017(5) -0.006(4) C11 0.048(6) 0.021(4) 0.035(5) 0.006(4) 0.026(4) 0.016(4) C12 0.027(5) 0.028(4) 0.030(5) -0.008(4) 0.008(4) 0.003(4) C13 0.031(4) 0.029(4) 0.042(5) 0.001(4) 0.021(4) -0.004(4) C14 0.032(5) 0.019(4) 0.039(5) 0.001(4) -0.013(4) 0.002(4) C15 0.041(6) 0.041(6) 0.033(5) -0.001(4) -0.005(5) 0.030(5) C16 0.020(4) 0.036(5) 0.047(6) 0.015(4) 0.005(4) 0.007(4) C17 0.037(5) 0.032(5) 0.031(5) -0.003(4) -0.003(4) 0.002(4) C18 0.038(5) 0.036(5) 0.038(6) 0.026(4) 0.001(4) 0.009(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C17 2.495(9) . ? Zr1 C13 2.514(8) . ? Zr1 C18 2.518(8) . ? Zr1 C16 2.528(8) . ? Zr1 C9 2.533(9) . ? Zr1 C10 2.534(8) . ? Zr1 C14 2.542(8) . ? Zr1 C15 2.553(8) . ? Zr1 C12 2.559(8) . ? Zr1 C11 2.560(8) . ? Zr1 P1 2.598(2) . ? Zr1 P1 2.612(2) 3_656 ? P1 P2 2.214(3) . ? P1 Zr1 2.612(2) 3_656 ? P2 N1 1.697(7) . ? P2 N2 1.703(7) . ? N1 C3 1.448(10) . ? N1 C1 1.464(10) . ? N2 C5 1.457(9) . ? N2 C7 1.480(9) . ? C1 C2 1.510(12) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 C4 1.535(12) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C6 1.494(11) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 C8 1.496(11) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C13 1.390(13) . ? C9 C10 1.406(14) . ? C9 H9 0.95 . ? C10 C11 1.380(13) . ? C10 H10 0.95 . ? C11 C12 1.374(12) . ? C11 H11 0.95 . ? C12 C13 1.410(12) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 C18 1.366(13) . ? C14 C15 1.385(14) . ? C14 H14 0.95 . ? C15 C16 1.385(14) . ? C15 H15 0.9501 . ? C16 C17 1.364(13) . ? C16 H16 0.95 . ? C17 C18 1.405(13) . ? C17 H17 0.9502 . ? C18 H18 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Zr1 C13 101.1(3) . . ? C17 Zr1 C18 32.5(3) . . ? C13 Zr1 C18 84.9(3) . . ? C17 Zr1 C16 31.5(3) . . ? C13 Zr1 C16 132.5(3) . . ? C18 Zr1 C16 52.8(3) . . ? C17 Zr1 C9 78.6(3) . . ? C13 Zr1 C9 32.0(3) . . ? C18 Zr1 C9 77.4(3) . . ? C16 Zr1 C9 108.5(3) . . ? C17 Zr1 C10 90.3(3) . . ? C13 Zr1 C10 53.8(3) . . ? C18 Zr1 C10 103.2(3) . . ? C16 Zr1 C10 110.5(3) . . ? C9 Zr1 C10 32.2(3) . . ? C17 Zr1 C14 52.7(3) . . ? C13 Zr1 C14 103.1(3) . . ? C18 Zr1 C14 31.3(3) . . ? C16 Zr1 C14 52.5(3) . . ? C9 Zr1 C14 106.3(3) . . ? C10 Zr1 C14 134.4(3) . . ? C17 Zr1 C15 52.2(3) . . ? C13 Zr1 C15 134.2(3) . . ? C18 Zr1 C15 52.1(3) . . ? C16 Zr1 C15 31.6(3) . . ? C9 Zr1 C15 127.7(3) . . ? C10 Zr1 C15 141.1(3) . . ? C14 Zr1 C15 31.6(3) . . ? C17 Zr1 C12 130.3(3) . . ? C13 Zr1 C12 32.3(3) . . ? C18 Zr1 C12 117.0(3) . . ? C16 Zr1 C12 160.5(3) . . ? C9 Zr1 C12 52.1(3) . . ? C10 Zr1 C12 52.5(3) . . ? C14 Zr1 C12 129.6(3) . . ? C15 Zr1 C12 159.7(3) . . ? C17 Zr1 C11 121.7(3) . . ? C13 Zr1 C11 52.9(3) . . ? C18 Zr1 C11 129.3(3) . . ? C16 Zr1 C11 138.0(3) . . ? C9 Zr1 C11 51.9(3) . . ? C10 Zr1 C11 31.4(3) . . ? C14 Zr1 C11 155.7(3) . . ? C15 Zr1 C11 168.9(3) . . ? C12 Zr1 C11 31.1(3) . . ? C17 Zr1 P1 135.8(2) . . ? C13 Zr1 P1 95.3(2) . . ? C18 Zr1 P1 110.8(2) . . ? C16 Zr1 P1 117.5(2) . . ? C9 Zr1 P1 127.1(2) . . ? C10 Zr1 P1 131.4(2) . . ? C14 Zr1 P1 83.8(2) . . ? C15 Zr1 P1 87.5(2) . . ? C12 Zr1 P1 81.0(2) . . ? C11 Zr1 P1 100.9(2) . . ? C17 Zr1 P1 105.9(2) . 3_656 ? C13 Zr1 P1 135.0(2) . 3_656 ? C18 Zr1 P1 134.4(2) . 3_656 ? C16 Zr1 P1 81.6(2) . 3_656 ? C9 Zr1 P1 122.5(3) . 3_656 ? C10 Zr1 P1 90.5(2) . 3_656 ? C14 Zr1 P1 121.8(2) . 3_656 ? C15 Zr1 P1 90.6(3) . 3_656 ? C12 Zr1 P1 105.9(2) . 3_656 ? C11 Zr1 P1 82.3(2) . 3_656 ? P1 Zr1 P1 89.70(7) . 3_656 ? P2 P1 Zr1 120.27(10) . . ? P2 P1 Zr1 115.18(10) . 3_656 ? Zr1 P1 Zr1 90.30(7) . 3_656 ? N1 P2 N2 109.6(3) . . ? N1 P2 P1 99.4(2) . . ? N2 P2 P1 101.2(2) . . ? C3 N1 C1 115.8(7) . . ? C3 N1 P2 118.4(5) . . ? C1 N1 P2 122.7(5) . . ? C5 N2 C7 115.0(6) . . ? C5 N2 P2 127.3(5) . . ? C7 N2 P2 116.9(5) . . ? N1 C1 C2 112.9(7) . . ? N1 C1 H1A 109 . . ? C2 C1 H1A 109 . . ? N1 C1 H1B 109 . . ? C2 C1 H1B 109 . . ? H1A C1 H1B 107.8 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 116.2(7) . . ? N1 C3 H3A 108.2 . . ? C4 C3 H3A 108.2 . . ? N1 C3 H3B 108.2 . . ? C4 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 114.0(7) . . ? N2 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 116.1(7) . . ? N2 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N2 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 C9 C10 109.5(8) . . ? C13 C9 Zr1 73.3(5) . . ? C10 C9 Zr1 74.0(5) . . ? C13 C9 H9 125.2 . . ? C10 C9 H9 125.2 . . ? Zr1 C9 H9 119.3 . . ? C11 C10 C9 106.3(8) . . ? C11 C10 Zr1 75.3(5) . . ? C9 C10 Zr1 73.8(5) . . ? C11 C10 H10 126.9 . . ? C9 C10 H10 126.9 . . ? Zr1 C10 H10 116.3 . . ? C12 C11 C10 109.6(8) . . ? C12 C11 Zr1 74.4(5) . . ? C10 C11 Zr1 73.2(5) . . ? C12 C11 H11 125.2 . . ? C10 C11 H11 125.2 . . ? Zr1 C11 H11 118.9 . . ? C11 C12 C13 108.4(8) . . ? C11 C12 Zr1 74.5(5) . . ? C13 C12 Zr1 72.1(5) . . ? C11 C12 H12 125.8 . . ? C13 C12 H12 125.8 . . ? Zr1 C12 H12 119.4 . . ? C9 C13 C12 106.0(8) . . ? C9 C13 Zr1 74.8(5) . . ? C12 C13 Zr1 75.6(5) . . ? C9 C13 H13 127 . . ? C12 C13 H13 127 . . ? Zr1 C13 H13 115.1 . . ? C18 C14 C15 108.1(8) . . ? C18 C14 Zr1 73.4(5) . . ? C15 C14 Zr1 74.6(5) . . ? C18 C14 H14 125.9 . . ? C15 C14 H14 125.9 . . ? Zr1 C14 H14 118 . . ? C16 C15 C14 108.2(9) . . ? C16 C15 Zr1 73.2(5) . . ? C14 C15 Zr1 73.8(5) . . ? C16 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? Zr1 C15 H15 119 . . ? C17 C16 C15 107.8(9) . . ? C17 C16 Zr1 72.9(5) . . ? C15 C16 Zr1 75.2(5) . . ? C17 C16 H16 126.1 . . ? C15 C16 H16 126.1 . . ? Zr1 C16 H16 117.8 . . ? C16 C17 C18 108.2(9) . . ? C16 C17 Zr1 75.6(5) . . ? C18 C17 Zr1 74.6(5) . . ? C16 C17 H17 125.9 . . ? C18 C17 H17 125.9 . . ? Zr1 C17 H17 116 . . ? C14 C18 C17 107.6(9) . . ? C14 C18 Zr1 75.3(5) . . ? C17 C18 Zr1 72.8(5) . . ? C14 C18 H18 126.2 . . ? C17 C18 H18 126.2 . . ? Zr1 C18 H18 117.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Zr1 P1 P2 -6.9(4) . . . . ? C13 Zr1 P1 P2 105.1(2) . . . . ? C18 Zr1 P1 P2 18.5(3) . . . . ? C16 Zr1 P1 P2 -39.4(3) . . . . ? C9 Zr1 P1 P2 108.2(3) . . . . ? C10 Zr1 P1 P2 149.8(3) . . . . ? C14 Zr1 P1 P2 2.4(3) . . . . ? C15 Zr1 P1 P2 -29.1(3) . . . . ? C12 Zr1 P1 P2 134.1(2) . . . . ? C11 Zr1 P1 P2 158.2(2) . . . . ? P1 Zr1 P1 P2 -119.72(13) 3_656 . . . ? C17 Zr1 P1 Zr1 112.8(3) . . . 3_656 ? C13 Zr1 P1 Zr1 -135.2(2) . . . 3_656 ? C18 Zr1 P1 Zr1 138.2(3) . . . 3_656 ? C16 Zr1 P1 Zr1 80.4(2) . . . 3_656 ? C9 Zr1 P1 Zr1 -132.1(3) . . . 3_656 ? C10 Zr1 P1 Zr1 -90.4(3) . . . 3_656 ? C14 Zr1 P1 Zr1 122.1(2) . . . 3_656 ? C15 Zr1 P1 Zr1 90.6(3) . . . 3_656 ? C12 Zr1 P1 Zr1 -106.2(2) . . . 3_656 ? C11 Zr1 P1 Zr1 -82.1(2) . . . 3_656 ? P1 Zr1 P1 Zr1 0 3_656 . . 3_656 ? Zr1 P1 P2 N1 178.9(2) . . . . ? Zr1 P1 P2 N1 72.6(2) 3_656 . . . ? Zr1 P1 P2 N2 -68.7(3) . . . . ? Zr1 P1 P2 N2 -175.1(2) 3_656 . . . ? N2 P2 N1 C3 106.1(6) . . . . ? P1 P2 N1 C3 -148.3(6) . . . . ? N2 P2 N1 C1 -52.8(7) . . . . ? P1 P2 N1 C1 52.8(6) . . . . ? N1 P2 N2 C5 65.7(7) . . . . ? P1 P2 N2 C5 -38.6(7) . . . . ? N1 P2 N2 C7 -103.3(6) . . . . ? P1 P2 N2 C7 152.3(5) . . . . ? C3 N1 C1 C2 59.7(9) . . . . ? P2 N1 C1 C2 -140.9(6) . . . . ? C1 N1 C3 C4 64.2(10) . . . . ? P2 N1 C3 C4 -96.2(8) . . . . ? C7 N2 C5 C6 -52.6(9) . . . . ? P2 N2 C5 C6 138.2(6) . . . . ? C5 N2 C7 C8 -55.2(10) . . . . ? P2 N2 C7 C8 115.2(7) . . . . ? C17 Zr1 C9 C13 134.1(6) . . . . ? C18 Zr1 C9 C13 100.8(6) . . . . ? C16 Zr1 C9 C13 144.0(5) . . . . ? C10 Zr1 C9 C13 -116.7(8) . . . . ? C14 Zr1 C9 C13 88.8(6) . . . . ? C15 Zr1 C9 C13 115.1(6) . . . . ? C12 Zr1 C9 C13 -39.0(5) . . . . ? C11 Zr1 C9 C13 -78.9(6) . . . . ? P1 Zr1 C9 C13 -5.9(7) . . . . ? P1 Zr1 C9 C13 -124.2(5) 3_656 . . . ? C17 Zr1 C9 C10 -109.2(6) . . . . ? C13 Zr1 C9 C10 116.7(8) . . . . ? C18 Zr1 C9 C10 -142.5(6) . . . . ? C16 Zr1 C9 C10 -99.3(6) . . . . ? C14 Zr1 C9 C10 -154.5(6) . . . . ? C15 Zr1 C9 C10 -128.1(6) . . . . ? C12 Zr1 C9 C10 77.7(6) . . . . ? C11 Zr1 C9 C10 37.8(5) . . . . ? P1 Zr1 C9 C10 110.8(5) . . . . ? P1 Zr1 C9 C10 -7.5(7) 3_656 . . . ? C13 C9 C10 C11 -3.8(10) . . . . ? Zr1 C9 C10 C11 -68.9(6) . . . . ? C13 C9 C10 Zr1 65.2(6) . . . . ? C17 Zr1 C10 C11 179.9(6) . . . . ? C13 Zr1 C10 C11 76.3(6) . . . . ? C18 Zr1 C10 C11 149.8(6) . . . . ? C16 Zr1 C10 C11 -155.4(5) . . . . ? C9 Zr1 C10 C11 112.2(8) . . . . ? C14 Zr1 C10 C11 147.5(5) . . . . ? C15 Zr1 C10 C11 -165.8(6) . . . . ? C12 Zr1 C10 C11 35.7(5) . . . . ? P1 Zr1 C10 C11 15.9(7) . . . . ? P1 Zr1 C10 C11 -74.1(5) 3_656 . . . ? C17 Zr1 C10 C9 67.8(6) . . . . ? C13 Zr1 C10 C9 -35.9(5) . . . . ? C18 Zr1 C10 C9 37.6(6) . . . . ? C16 Zr1 C10 C9 92.4(6) . . . . ? C14 Zr1 C10 C9 35.3(7) . . . . ? C15 Zr1 C10 C9 82.0(7) . . . . ? C12 Zr1 C10 C9 -76.5(6) . . . . ? C11 Zr1 C10 C9 -112.2(8) . . . . ? P1 Zr1 C10 C9 -96.3(6) . . . . ? P1 Zr1 C10 C9 173.7(6) 3_656 . . . ? C9 C10 C11 C12 1.8(9) . . . . ? Zr1 C10 C11 C12 -66.0(6) . . . . ? C9 C10 C11 Zr1 67.9(6) . . . . ? C17 Zr1 C11 C12 116.6(6) . . . . ? C13 Zr1 C11 C12 37.1(5) . . . . ? C18 Zr1 C11 C12 77.3(7) . . . . ? C16 Zr1 C11 C12 152.3(5) . . . . ? C9 Zr1 C11 C12 77.8(6) . . . . ? C10 Zr1 C11 C12 116.6(8) . . . . ? C14 Zr1 C11 C12 47.8(10) . . . . ? C15 Zr1 C11 C12 170.1(14) . . . . ? P1 Zr1 C11 C12 -51.3(5) . . . . ? P1 Zr1 C11 C12 -139.5(5) 3_656 . . . ? C17 Zr1 C11 C10 -0.1(7) . . . . ? C13 Zr1 C11 C10 -79.5(6) . . . . ? C18 Zr1 C11 C10 -39.3(7) . . . . ? C16 Zr1 C11 C10 35.7(7) . . . . ? C9 Zr1 C11 C10 -38.9(5) . . . . ? C14 Zr1 C11 C10 -68.8(10) . . . . ? C15 Zr1 C11 C10 53.4(17) . . . . ? C12 Zr1 C11 C10 -116.6(8) . . . . ? P1 Zr1 C11 C10 -167.9(5) . . . . ? P1 Zr1 C11 C10 103.9(5) 3_656 . . . ? C10 C11 C12 C13 0.7(9) . . . . ? Zr1 C11 C12 C13 -64.6(6) . . . . ? C10 C11 C12 Zr1 65.3(6) . . . . ? C17 Zr1 C12 C11 -86.0(6) . . . . ? C13 Zr1 C12 C11 -115.8(8) . . . . ? C18 Zr1 C12 C11 -122.0(6) . . . . ? C16 Zr1 C12 C11 -68.4(10) . . . . ? C9 Zr1 C12 C11 -77.1(6) . . . . ? C10 Zr1 C12 C11 -36.0(5) . . . . ? C14 Zr1 C12 C11 -156.7(5) . . . . ? C15 Zr1 C12 C11 -174.5(8) . . . . ? P1 Zr1 C12 C11 129.1(5) . . . . ? P1 Zr1 C12 C11 42.0(5) 3_656 . . . ? C17 Zr1 C12 C13 29.8(6) . . . . ? C18 Zr1 C12 C13 -6.3(6) . . . . ? C16 Zr1 C12 C13 47.3(11) . . . . ? C9 Zr1 C12 C13 38.7(5) . . . . ? C10 Zr1 C12 C13 79.8(6) . . . . ? C14 Zr1 C12 C13 -40.9(6) . . . . ? C15 Zr1 C12 C13 -58.8(10) . . . . ? C11 Zr1 C12 C13 115.8(8) . . . . ? P1 Zr1 C12 C13 -115.1(5) . . . . ? P1 Zr1 C12 C13 157.8(5) 3_656 . . . ? C10 C9 C13 C12 4.2(10) . . . . ? Zr1 C9 C13 C12 69.8(6) . . . . ? C10 C9 C13 Zr1 -65.6(6) . . . . ? C11 C12 C13 C9 -3.0(9) . . . . ? Zr1 C12 C13 C9 -69.2(6) . . . . ? C11 C12 C13 Zr1 66.2(6) . . . . ? C17 Zr1 C13 C9 -45.9(6) . . . . ? C18 Zr1 C13 C9 -74.2(6) . . . . ? C16 Zr1 C13 C9 -49.1(7) . . . . ? C10 Zr1 C13 C9 36.2(6) . . . . ? C14 Zr1 C13 C9 -99.8(6) . . . . ? C15 Zr1 C13 C9 -93.1(7) . . . . ? C12 Zr1 C13 C9 111.4(8) . . . . ? C11 Zr1 C13 C9 75.6(6) . . . . ? P1 Zr1 C13 C9 175.3(5) . . . . ? P1 Zr1 C13 C9 80.5(6) 3_656 . . . ? C17 Zr1 C13 C12 -157.3(5) . . . . ? C18 Zr1 C13 C12 174.4(5) . . . . ? C16 Zr1 C13 C12 -160.5(5) . . . . ? C9 Zr1 C13 C12 -111.4(8) . . . . ? C10 Zr1 C13 C12 -75.2(6) . . . . ? C14 Zr1 C13 C12 148.8(5) . . . . ? C15 Zr1 C13 C12 155.5(5) . . . . ? C11 Zr1 C13 C12 -35.8(5) . . . . ? P1 Zr1 C13 C12 63.9(5) . . . . ? P1 Zr1 C13 C12 -30.9(6) 3_656 . . . ? C17 Zr1 C14 C18 -38.1(6) . . . . ? C13 Zr1 C14 C18 56.0(6) . . . . ? C16 Zr1 C14 C18 -78.1(6) . . . . ? C9 Zr1 C14 C18 23.0(7) . . . . ? C10 Zr1 C14 C18 4.3(8) . . . . ? C15 Zr1 C14 C18 -114.8(8) . . . . ? C12 Zr1 C14 C18 77.0(7) . . . . ? C11 Zr1 C14 C18 47.2(10) . . . . ? P1 Zr1 C14 C18 149.9(6) . . . . ? P1 Zr1 C14 C18 -124.3(6) 3_656 . . . ? C17 Zr1 C14 C15 76.6(6) . . . . ? C13 Zr1 C14 C15 170.7(5) . . . . ? C18 Zr1 C14 C15 114.8(8) . . . . ? C16 Zr1 C14 C15 36.7(5) . . . . ? C9 Zr1 C14 C15 137.8(6) . . . . ? C10 Zr1 C14 C15 119.1(6) . . . . ? C12 Zr1 C14 C15 -168.2(5) . . . . ? C11 Zr1 C14 C15 161.9(7) . . . . ? P1 Zr1 C14 C15 -95.3(5) . . . . ? P1 Zr1 C14 C15 -9.5(6) 3_656 . . . ? C18 C14 C15 C16 0.6(10) . . . . ? Zr1 C14 C15 C16 -65.6(6) . . . . ? C18 C14 C15 Zr1 66.3(6) . . . . ? C17 Zr1 C15 C16 37.0(5) . . . . ? C13 Zr1 C15 C16 102.7(7) . . . . ? C18 Zr1 C15 C16 78.6(6) . . . . ? C9 Zr1 C15 C16 60.8(7) . . . . ? C10 Zr1 C15 C16 18.9(9) . . . . ? C14 Zr1 C15 C16 115.3(8) . . . . ? C12 Zr1 C15 C16 142.2(8) . . . . ? C11 Zr1 C15 C16 -22.9(19) . . . . ? P1 Zr1 C15 C16 -162.4(6) . . . . ? P1 Zr1 C15 C16 -72.7(6) 3_656 . . . ? C17 Zr1 C15 C14 -78.3(6) . . . . ? C13 Zr1 C15 C14 -12.6(7) . . . . ? C18 Zr1 C15 C14 -36.7(5) . . . . ? C16 Zr1 C15 C14 -115.3(8) . . . . ? C9 Zr1 C15 C14 -54.6(7) . . . . ? C10 Zr1 C15 C14 -96.5(7) . . . . ? C12 Zr1 C15 C14 26.9(11) . . . . ? C11 Zr1 C15 C14 -138.2(15) . . . . ? P1 Zr1 C15 C14 82.2(5) . . . . ? P1 Zr1 C15 C14 171.9(5) 3_656 . . . ? C14 C15 C16 C17 -0.1(10) . . . . ? Zr1 C15 C16 C17 -66.1(6) . . . . ? C14 C15 C16 Zr1 66.0(6) . . . . ? C13 Zr1 C16 C17 6.1(7) . . . . ? C18 Zr1 C16 C17 38.1(6) . . . . ? C9 Zr1 C16 C17 -18.9(6) . . . . ? C10 Zr1 C16 C17 -53.1(6) . . . . ? C14 Zr1 C16 C17 77.8(6) . . . . ? C15 Zr1 C16 C17 114.4(9) . . . . ? C12 Zr1 C16 C17 -26.1(12) . . . . ? C11 Zr1 C16 C17 -72.0(7) . . . . ? P1 Zr1 C16 C17 134.3(5) . . . . ? P1 Zr1 C16 C17 -140.5(6) 3_656 . . . ? C17 Zr1 C16 C15 -114.4(9) . . . . ? C13 Zr1 C16 C15 -108.3(7) . . . . ? C18 Zr1 C16 C15 -76.2(7) . . . . ? C9 Zr1 C16 C15 -133.3(6) . . . . ? C10 Zr1 C16 C15 -167.5(6) . . . . ? C14 Zr1 C16 C15 -36.6(6) . . . . ? C12 Zr1 C16 C15 -140.4(8) . . . . ? C11 Zr1 C16 C15 173.6(6) . . . . ? P1 Zr1 C16 C15 19.9(7) . . . . ? P1 Zr1 C16 C15 105.1(6) 3_656 . . . ? C15 C16 C17 C18 -0.4(10) . . . . ? Zr1 C16 C17 C18 -68.1(6) . . . . ? C15 C16 C17 Zr1 67.7(6) . . . . ? C13 Zr1 C17 C16 -175.4(6) . . . . ? C18 Zr1 C17 C16 -113.9(9) . . . . ? C9 Zr1 C17 C16 161.8(6) . . . . ? C10 Zr1 C17 C16 131.5(6) . . . . ? C14 Zr1 C17 C16 -77.3(6) . . . . ? C15 Zr1 C17 C16 -37.2(6) . . . . ? C12 Zr1 C17 C16 168.9(5) . . . . ? C11 Zr1 C17 C16 131.6(6) . . . . ? P1 Zr1 C17 C16 -65.7(7) . . . . ? P1 Zr1 C17 C16 40.9(6) 3_656 . . . ? C13 Zr1 C17 C18 -61.5(6) . . . . ? C16 Zr1 C17 C18 113.9(9) . . . . ? C9 Zr1 C17 C18 -84.3(6) . . . . ? C10 Zr1 C17 C18 -114.6(6) . . . . ? C14 Zr1 C17 C18 36.6(6) . . . . ? C15 Zr1 C17 C18 76.7(7) . . . . ? C12 Zr1 C17 C18 -77.2(7) . . . . ? C11 Zr1 C17 C18 -114.5(6) . . . . ? P1 Zr1 C17 C18 48.2(7) . . . . ? P1 Zr1 C17 C18 154.8(6) 3_656 . . . ? C15 C14 C18 C17 -0.9(10) . . . . ? Zr1 C14 C18 C17 66.2(6) . . . . ? C15 C14 C18 Zr1 -67.1(6) . . . . ? C16 C17 C18 C14 0.8(10) . . . . ? Zr1 C17 C18 C14 -67.9(6) . . . . ? C16 C17 C18 Zr1 68.8(6) . . . . ? C17 Zr1 C18 C14 114.1(9) . . . . ? C13 Zr1 C18 C14 -125.9(6) . . . . ? C16 Zr1 C18 C14 77.2(6) . . . . ? C9 Zr1 C18 C14 -157.4(6) . . . . ? C10 Zr1 C18 C14 -176.8(6) . . . . ? C15 Zr1 C18 C14 37.0(6) . . . . ? C12 Zr1 C18 C14 -122.5(6) . . . . ? C11 Zr1 C18 C14 -157.0(6) . . . . ? P1 Zr1 C18 C14 -32.2(6) . . . . ? P1 Zr1 C18 C14 79.1(6) 3_656 . . . ? C13 Zr1 C18 C17 120.1(6) . . . . ? C16 Zr1 C18 C17 -36.8(6) . . . . ? C9 Zr1 C18 C17 88.6(6) . . . . ? C10 Zr1 C18 C17 69.1(6) . . . . ? C14 Zr1 C18 C17 -114.1(9) . . . . ? C15 Zr1 C18 C17 -77.0(6) . . . . ? C12 Zr1 C18 C17 123.4(6) . . . . ? C11 Zr1 C18 C17 88.9(7) . . . . ? P1 Zr1 C18 C17 -146.3(5) . . . . ? P1 Zr1 C18 C17 -34.9(7) 3_656 . . . ? # END of CIF _chemical_name_common ; Bis(mu-(bi(diethylamino)phosphinephosphinideno)-bis- cyclopentadienylo zirconium(IV)) ; data_ola1k _database_code_depnum_ccdc_archive 'CCDC 787635' #TrackingRef '- ola1k_doCCDC.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2010-07-31 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ; FM 2010-08-03 # Formatted by publCIF ; _vrf_REFLT03_ola1k ; PROBLEM: Reflection count > 15% excess reflns - sys abs data present? RESPONSE: The structure has a 21% twin component related a by 180\% rotation about the [1-12] reciprocal lattice direction. The twinning was resolved with the aid of the program TwinRotMat option in PLATON. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; {(Bis-diethylaminophosphanyl)(trimethylsilyl)phosphide}(chlorido) (bis-cyclopentadienylo) hafnium(IV) ; _chemical_formula_moiety 'C21 H39 Cl Hf N2 P2 Si' _chemical_formula_sum 'C21 H39 Cl Hf N2 P2 Si' _chemical_formula_weight 623.51 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0239(17) _cell_length_b 15.008(2) _cell_length_c 16.892(3) _cell_angle_alpha 71.665(14) _cell_angle_beta 78.786(13) _cell_angle_gamma 81.294(13) _cell_volume 2590.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7306 _cell_measurement_theta_min 2.2163 _cell_measurement_theta_max 32.4603 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1707 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_min 0.0538 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.311 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED (Oxford Diffraction, 2006) ; _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_T_max 0.622 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.1883 _diffrn_orient_matrix_ub_11 0.0194156347 _diffrn_orient_matrix_ub_12 -0.0309675403 _diffrn_orient_matrix_ub_13 0.0377883531 _diffrn_orient_matrix_ub_21 -0.0436564862 _diffrn_orient_matrix_ub_22 0.0251161659 _diffrn_orient_matrix_ub_23 0.0242163641 _diffrn_orient_matrix_ub_31 -0.0457491499 _diffrn_orient_matrix_ub_32 -0.030150535 _diffrn_orient_matrix_ub_33 0.0032727192 _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire2 (large Be window)' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0962 _diffrn_reflns_av_unetI/netI 0.1169 _diffrn_reflns_number 17964 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 17964 _reflns_number_gt 11025 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2006) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 17964 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1372 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.2462 _refine_ls_wR_factor_gt 0.2156 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.06 _refine_diff_density_min -1.775 _refine_diff_density_rms 0.315 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.583 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7038(14) 0.5018(10) 0.0087(9) 0.025(3) Uani 1 1 d . . . H1 H 0.7134 0.5591 0.0185 0.03 Uiso 1 1 calc R . . C2 C 0.6119(12) 0.4410(9) 0.0529(9) 0.023(3) Uani 1 1 d . . . H2 H 0.5484 0.4497 0.0975 0.027 Uiso 1 1 calc R . . C3 C 0.6321(14) 0.3637(9) 0.0179(9) 0.026(3) Uani 1 1 d . . . H3 H 0.5849 0.3109 0.0362 0.032 Uiso 1 1 calc R . . C4 C 0.7356(13) 0.3794(11) -0.0494(9) 0.028(3) Uani 1 1 d . . . H4 H 0.7676 0.3402 -0.0848 0.033 Uiso 1 1 calc R . . C5 C 0.7805(13) 0.4631(11) -0.0533(10) 0.027(3) Uani 1 1 d . . . H5 H 0.8504 0.4899 -0.091 0.033 Uiso 1 1 calc R . . C6 C 0.9183(13) 0.2177(10) 0.0330(10) 0.030(4) Uani 1 1 d . . . H6 H 0.8697 0.1923 0.0061 0.036 Uiso 1 1 calc R . . C7 C 0.9249(14) 0.1889(10) 0.1214(9) 0.029(3) Uani 1 1 d . . . H7 H 0.8831 0.14 0.1635 0.035 Uiso 1 1 calc R . . C8 C 1.0046(13) 0.2461(10) 0.1346(10) 0.027(3) Uani 1 1 d . . . H8 H 1.025 0.2441 0.1873 0.033 Uiso 1 1 calc R . . C9 C 1.0495(14) 0.3083(11) 0.0531(10) 0.035(4) Uani 1 1 d . . . H9 H 1.1061 0.3538 0.0433 0.042 Uiso 1 1 calc R . . C10 C 0.9984(12) 0.2918(10) -0.0082(9) 0.024(3) Uani 1 1 d . . . H10 H 1.0132 0.3234 -0.067 0.029 Uiso 1 1 calc R . . C11 C 0.5118(16) 0.0789(12) 0.3039(10) 0.040(4) Uani 1 1 d . . . H11A H 0.4565 0.0401 0.2932 0.061 Uiso 1 1 calc R . . H11B H 0.4713 0.1025 0.3514 0.061 Uiso 1 1 calc R . . H11C H 0.5895 0.0407 0.3176 0.061 Uiso 1 1 calc R . . C12 C 0.3955(12) 0.2555(10) 0.1778(10) 0.027(3) Uani 1 1 d . . . H12A H 0.3432 0.2168 0.164 0.041 Uiso 1 1 calc R . . H12B H 0.414 0.3104 0.1289 0.041 Uiso 1 1 calc R . . H12C H 0.3515 0.2767 0.2259 0.041 Uiso 1 1 calc R . . C13 C 0.6127(14) 0.1252(10) 0.1221(9) 0.028(3) Uani 1 1 d . . . H13A H 0.6746 0.0731 0.143 0.042 Uiso 1 1 calc R . . H13B H 0.6522 0.1716 0.0725 0.042 Uiso 1 1 calc R . . H13C H 0.546 0.1008 0.1066 0.042 Uiso 1 1 calc R . . C14 C 0.6497(15) 0.0710(11) 0.4764(10) 0.037(4) Uani 1 1 d . . . H14A H 0.678 0.0213 0.448 0.048 Uiso 1 1 calc R . . H14B H 0.5643 0.0603 0.5067 0.048 Uiso 1 1 calc R . . C15 C 0.7347(18) 0.0614(12) 0.5407(13) 0.054(5) Uani 1 1 d . . . H15A H 0.8215 0.0597 0.5131 0.081 Uiso 1 1 calc R . . H15B H 0.7221 0.003 0.5868 0.081 Uiso 1 1 calc R . . H15C H 0.715 0.1154 0.5633 0.081 Uiso 1 1 calc R . . C16 C 0.5691(14) 0.2414(12) 0.4373(10) 0.035(4) Uani 1 1 d . . . H16A H 0.5917 0.3028 0.3973 0.045 Uiso 1 1 calc R . . H16B H 0.5852 0.239 0.4936 0.045 Uiso 1 1 calc R . . C17 C 0.4307(16) 0.2343(15) 0.4419(14) 0.058(6) Uani 1 1 d . . . H17A H 0.4137 0.2397 0.3857 0.086 Uiso 1 1 calc R . . H17B H 0.3817 0.2852 0.462 0.086 Uiso 1 1 calc R . . H17C H 0.4081 0.1733 0.481 0.086 Uiso 1 1 calc R . . C18 C 0.8449(14) 0.3376(10) 0.3460(9) 0.027(3) Uani 1 1 d . . . H18A H 0.9128 0.3769 0.3135 0.035 Uiso 1 1 calc R . . H18B H 0.768 0.3674 0.3225 0.035 Uiso 1 1 calc R . . C19 C 0.8269(15) 0.3377(11) 0.4381(10) 0.033(4) Uani 1 1 d . . . H19A H 0.7667 0.2932 0.4723 0.049 Uiso 1 1 calc R . . H19B H 0.7959 0.4012 0.4419 0.049 Uiso 1 1 calc R . . H19C H 0.9065 0.3186 0.4592 0.049 Uiso 1 1 calc R . . C20 C 0.9831(12) 0.1873(11) 0.3736(9) 0.028(3) Uani 1 1 d . . . H20A H 1.0001 0.1251 0.3629 0.036 Uiso 1 1 calc R . . H20B H 0.9612 0.1761 0.4354 0.036 Uiso 1 1 calc R . . C21 C 1.1040(14) 0.2390(11) 0.3418(12) 0.038(4) Uani 1 1 d . . . H21A H 1.1272 0.2498 0.2808 0.057 Uiso 1 1 calc R . . H21B H 1.1714 0.2 0.3706 0.057 Uiso 1 1 calc R . . H21C H 1.0892 0.2997 0.3542 0.057 Uiso 1 1 calc R . . C22 C 0.5430(13) 0.8173(11) 0.1171(11) 0.034(4) Uani 1 1 d . . . H22 H 0.5131 0.8804 0.1159 0.041 Uiso 1 1 calc R . . C23 C 0.6694(13) 0.7709(11) 0.1255(9) 0.026(3) Uani 1 1 d . . . H23 H 0.7372 0.8011 0.1288 0.031 Uiso 1 1 calc R . . C24 C 0.6755(14) 0.6809(11) 0.1280(9) 0.029(3) Uani 1 1 d . . . H24 H 0.7474 0.6369 0.1327 0.034 Uiso 1 1 calc R . . C25 C 0.5542(14) 0.6620(11) 0.1223(10) 0.033(4) Uani 1 1 d . . . H25 H 0.5291 0.6031 0.1251 0.039 Uiso 1 1 calc R . . C26 C 0.4789(15) 0.7499(12) 0.1115(9) 0.035(4) Uani 1 1 d . . . H26 H 0.3952 0.7598 0.1017 0.042 Uiso 1 1 calc R . . C27 C 0.7010(14) 0.5768(12) 0.3119(10) 0.034(4) Uani 1 1 d . . . H27 H 0.7799 0.5805 0.277 0.041 Uiso 1 1 calc R . . C28 C 0.6058(14) 0.5257(10) 0.3091(10) 0.033(4) Uani 1 1 d . . . H28 H 0.6082 0.4888 0.2722 0.039 Uiso 1 1 calc R . . C29 C 0.5072(13) 0.5396(9) 0.3709(10) 0.025(3) Uani 1 1 d . . . H29 H 0.4306 0.5128 0.383 0.03 Uiso 1 1 calc R . . C30 C 0.5366(16) 0.5985(10) 0.4124(9) 0.033(4) Uani 1 1 d . . . H30 H 0.485 0.619 0.4567 0.04 Uiso 1 1 calc R . . C31 C 0.6593(15) 0.6218(11) 0.3753(10) 0.037(4) Uani 1 1 d . . . H31 H 0.7052 0.6608 0.3906 0.045 Uiso 1 1 calc R . . C32 C 0.1672(13) 0.4973(10) 0.4289(9) 0.027(3) Uani 1 1 d . . . H32A H 0.1133 0.5401 0.4571 0.041 Uiso 1 1 calc R . . H32B H 0.2436 0.4767 0.4538 0.041 Uiso 1 1 calc R . . H32C H 0.1239 0.4423 0.4359 0.041 Uiso 1 1 calc R . . C33 C 0.3108(13) 0.4795(10) 0.2587(9) 0.024(3) Uani 1 1 d . . . H33A H 0.268 0.4244 0.2651 0.036 Uiso 1 1 calc R . . H33B H 0.3873 0.4589 0.2836 0.036 Uiso 1 1 calc R . . H33C H 0.3314 0.5132 0.1986 0.036 Uiso 1 1 calc R . . C34 C 0.0554(14) 0.5833(10) 0.2700(10) 0.031(4) Uani 1 1 d . . . H34A H 0.0685 0.6222 0.2109 0.046 Uiso 1 1 calc R . . H34B H -0.0076 0.6165 0.303 0.046 Uiso 1 1 calc R . . H34C H 0.027 0.5233 0.2734 0.046 Uiso 1 1 calc R . . C35 C -0.0751(13) 0.8226(10) 0.2288(11) 0.031(4) Uani 1 1 d . . . H35A H -0.1364 0.7805 0.2674 0.038 Uiso 1 1 calc R . . H35B H -0.0563 0.8051 0.1756 0.038 Uiso 1 1 calc R . . C36 C -0.1381(14) 0.9213(10) 0.2090(12) 0.038(4) Uani 1 1 d . . . H36A H -0.1534 0.9424 0.2597 0.057 Uiso 1 1 calc R . . H36B H -0.2173 0.9225 0.1904 0.057 Uiso 1 1 calc R . . H36C H -0.0847 0.9635 0.1641 0.057 Uiso 1 1 calc R . . C37 C 0.0182(13) 0.8211(11) 0.3486(9) 0.028(3) Uani 1 1 d . . . H37A H -0.0038 0.8896 0.3399 0.033 Uiso 1 1 calc R . . H37B H 0.097 0.8032 0.3719 0.033 Uiso 1 1 calc R . . C38 C -0.0837(14) 0.7671(12) 0.4113(10) 0.035(4) Uani 1 1 d . . . H38A H -0.1511 0.8118 0.4274 0.052 Uiso 1 1 calc R . . H38B H -0.0497 0.727 0.4616 0.052 Uiso 1 1 calc R . . H38C H -0.1161 0.7277 0.3852 0.052 Uiso 1 1 calc R . . C39 C 0.2632(18) 0.9528(13) 0.0810(9) 0.046(5) Uani 1 1 d . . . H39A H 0.3223 0.9996 0.0732 0.055 Uiso 1 1 calc R . . H39B H 0.304 0.9091 0.0483 0.055 Uiso 1 1 calc R . . C40 C 0.1562(18) 1.0025(12) 0.0439(11) 0.048(5) Uani 1 1 d . . . H40A H 0.0846 0.9659 0.0692 0.072 Uiso 1 1 calc R . . H40B H 0.173 1.0114 -0.0171 0.072 Uiso 1 1 calc R . . H40C H 0.1382 1.0642 0.0544 0.072 Uiso 1 1 calc R . . C41 C 0.2677(13) 0.9458(10) 0.2308(10) 0.028(3) Uani 1 1 d . . . H41A H 0.3545 0.9622 0.2144 0.034 Uiso 1 1 calc R . . H41B H 0.2603 0.9012 0.2885 0.034 Uiso 1 1 calc R . . C42 C 0.1855(14) 1.0327(10) 0.2338(9) 0.027(3) Uani 1 1 d . . . H42A H 0.1967 1.0799 0.1783 0.041 Uiso 1 1 calc R . . H42B H 0.2066 1.0576 0.2761 0.041 Uiso 1 1 calc R . . H42C H 0.0987 1.0182 0.2492 0.041 Uiso 1 1 calc R . . N1 N 0.6465(11) 0.1660(8) 0.4101(7) 0.024(3) Uani 1 1 d . . . N2 N 0.8756(10) 0.2398(9) 0.3332(7) 0.027(3) Uani 1 1 d . . . N3 N 0.0359(10) 0.8009(7) 0.2651(7) 0.018(2) Uiso 1 1 d . . . N4 N 0.2446(11) 0.8966(8) 0.1733(7) 0.023(3) Uani 1 1 d . . . Si1 Si 0.5468(4) 0.1824(3) 0.2061(3) 0.0245(9) Uani 1 1 d . . . Si2 Si 0.2069(4) 0.5601(3) 0.3139(3) 0.0222(9) Uani 1 1 d . . . P1 P 0.6680(3) 0.2804(2) 0.2257(2) 0.0185(8) Uani 1 1 d . . . P2 P 0.7667(3) 0.1775(3) 0.3263(2) 0.0209(8) Uani 1 1 d . . . P3 P 0.2862(3) 0.6965(3) 0.2999(2) 0.0217(8) Uani 1 1 d . . . P4 P 0.1772(3) 0.7942(3) 0.2028(2) 0.0220(8) Uani 1 1 d . . . Cl1 Cl 0.8951(3) 0.4651(2) 0.1342(2) 0.0231(7) Uani 1 1 d . . . Cl2 Cl 0.5503(3) 0.8300(3) 0.3023(2) 0.0289(8) Uani 1 1 d . . . Hf1 Hf 0.82046(5) 0.35111(4) 0.08469(3) 0.01728(17) Uani 1 1 d . . . Hf2 Hf 0.52975(5) 0.69517(4) 0.25893(4) 0.02075(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(9) 0.023(8) 0.022(7) -0.011(6) -0.011(7) 0.000(6) C2 0.016(7) 0.024(8) 0.020(7) -0.003(6) -0.001(6) 0.012(6) C3 0.037(9) 0.016(7) 0.025(8) 0.007(6) -0.019(7) -0.008(6) C4 0.023(8) 0.040(9) 0.033(8) -0.024(7) -0.014(7) 0.000(7) C5 0.017(8) 0.035(9) 0.039(9) -0.019(7) -0.014(7) 0.002(6) C6 0.022(8) 0.034(9) 0.045(9) -0.035(8) -0.002(7) 0.009(6) C7 0.033(9) 0.023(8) 0.028(8) -0.005(7) -0.007(7) 0.010(6) C8 0.021(8) 0.031(9) 0.029(8) -0.009(7) -0.004(7) 0.002(6) C9 0.024(8) 0.029(9) 0.047(10) -0.015(8) -0.007(8) 0.018(7) C10 0.016(7) 0.026(8) 0.029(8) -0.015(7) 0.006(6) 0.002(6) C11 0.040(10) 0.061(12) 0.031(9) -0.028(9) -0.009(8) -0.005(8) C12 0.017(8) 0.032(9) 0.036(9) -0.011(7) -0.005(7) -0.007(6) C13 0.038(9) 0.021(8) 0.027(8) -0.012(7) -0.012(7) 0.007(6) C14 0.041(10) 0.026(9) 0.035(9) 0.007(7) -0.014(8) 0.003(7) C15 0.071(14) 0.022(9) 0.068(13) -0.004(9) -0.034(11) 0.013(8) C16 0.028(9) 0.054(11) 0.024(8) -0.015(8) 0.004(7) -0.010(7) C17 0.033(10) 0.075(15) 0.081(15) -0.052(13) -0.004(10) 0.001(9) C18 0.040(9) 0.022(8) 0.029(8) -0.015(7) -0.021(7) 0.004(6) C19 0.044(10) 0.025(8) 0.033(9) -0.012(7) -0.014(7) 0.006(7) C20 0.012(7) 0.044(10) 0.027(8) -0.011(7) -0.002(6) -0.001(6) C21 0.031(9) 0.028(9) 0.064(12) -0.020(8) -0.011(8) -0.015(7) C22 0.022(8) 0.023(8) 0.054(10) -0.009(8) -0.009(8) 0.009(6) C23 0.017(8) 0.037(9) 0.027(8) -0.005(7) -0.008(6) -0.016(6) C24 0.027(8) 0.033(9) 0.028(8) -0.014(7) -0.004(7) 0.000(7) C25 0.028(9) 0.038(9) 0.048(10) -0.034(8) 0.000(7) -0.011(7) C26 0.039(10) 0.055(11) 0.014(7) -0.016(8) -0.007(7) 0.005(8) C27 0.023(8) 0.056(11) 0.026(8) -0.014(8) -0.020(7) 0.015(7) C28 0.036(9) 0.022(8) 0.040(9) -0.008(7) -0.021(8) 0.012(7) C29 0.017(7) 0.020(7) 0.047(9) -0.023(7) -0.007(7) 0.001(6) C30 0.053(11) 0.023(8) 0.024(8) -0.004(7) -0.022(8) 0.013(7) C31 0.042(10) 0.034(9) 0.043(10) -0.011(8) -0.032(9) 0.007(7) C32 0.017(8) 0.026(8) 0.036(9) -0.002(7) -0.008(7) -0.003(6) C33 0.026(8) 0.031(8) 0.025(8) -0.014(7) -0.017(6) -0.003(6) C34 0.033(9) 0.025(8) 0.047(10) -0.018(7) -0.022(8) -0.002(6) C35 0.025(8) 0.026(8) 0.055(10) -0.026(8) -0.014(8) 0.001(6) C36 0.023(8) 0.016(8) 0.068(12) -0.009(8) -0.009(8) 0.011(6) C37 0.016(7) 0.037(9) 0.041(9) -0.028(8) -0.008(7) 0.004(6) C38 0.030(9) 0.050(11) 0.036(9) -0.021(8) -0.005(7) -0.021(8) C39 0.073(13) 0.047(11) 0.015(8) -0.009(8) -0.012(8) 0.014(9) C40 0.068(13) 0.036(10) 0.037(10) -0.008(8) -0.010(9) -0.001(9) C41 0.026(8) 0.028(8) 0.031(8) -0.001(7) -0.020(7) 0.002(6) C42 0.038(9) 0.022(8) 0.029(8) -0.017(7) -0.018(7) 0.011(6) N1 0.029(7) 0.017(6) 0.031(7) -0.012(5) -0.010(6) -0.002(5) N2 0.011(6) 0.050(8) 0.016(6) -0.001(6) -0.002(5) -0.009(5) N4 0.029(7) 0.025(7) 0.021(6) -0.012(5) -0.011(5) 0.003(5) Si1 0.026(2) 0.022(2) 0.029(2) -0.0112(18) -0.0050(18) -0.0032(16) Si2 0.024(2) 0.017(2) 0.028(2) -0.0109(17) -0.0063(17) 0.0027(16) P1 0.0201(19) 0.0175(18) 0.0192(18) -0.0077(15) -0.0027(15) -0.0006(14) P2 0.0217(19) 0.0178(18) 0.0238(19) -0.0079(15) 0.0001(15) -0.0049(14) P3 0.0177(19) 0.023(2) 0.025(2) -0.0096(16) -0.0056(16) 0.0030(14) P4 0.0207(19) 0.023(2) 0.028(2) -0.0139(16) -0.0075(16) 0.0011(15) Cl1 0.0278(19) 0.0203(17) 0.0249(17) -0.0094(15) -0.0078(15) -0.0032(14) Cl2 0.029(2) 0.029(2) 0.033(2) -0.0148(16) -0.0093(16) -0.0002(15) Hf1 0.0176(3) 0.0174(3) 0.0185(3) -0.0079(2) -0.0044(2) 0.0007(2) Hf2 0.0186(3) 0.0214(3) 0.0262(4) -0.0124(3) -0.0078(3) 0.0035(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.404(19) . ? C1 C5 1.43(2) . ? C1 Hf1 2.520(14) . ? C1 H1 0.95 . ? C2 C3 1.43(2) . ? C2 Hf1 2.546(13) . ? C2 H2 0.95 . ? C3 C4 1.44(2) . ? C3 Hf1 2.506(13) . ? C3 H3 0.95 . ? C4 C5 1.40(2) . ? C4 Hf1 2.508(14) . ? C4 H4 0.95 . ? C5 Hf1 2.483(15) . ? C5 H5 0.95 . ? C6 C7 1.43(2) . ? C6 C10 1.44(2) . ? C6 Hf1 2.454(13) . ? C6 H6 0.95 . ? C7 C8 1.41(2) . ? C7 Hf1 2.474(14) . ? C7 H7 0.95 . ? C8 C9 1.44(2) . ? C8 Hf1 2.486(14) . ? C8 H8 0.95 . ? C9 C10 1.37(2) . ? C9 Hf1 2.505(14) . ? C9 H9 0.95 . ? C10 Hf1 2.501(13) . ? C10 H10 0.95 . ? C11 Si1 1.900(17) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 Si1 1.909(14) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 Si1 1.857(14) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 N1 1.511(18) . ? C14 C15 1.53(2) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 N1 1.449(19) . ? C16 C17 1.53(2) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.53(2) . ? C18 N2 1.530(18) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 N2 1.478(18) . ? C20 C21 1.561(19) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C26 1.35(2) . ? C22 C23 1.47(2) . ? C22 Hf2 2.510(16) . ? C22 H22 0.95 . ? C23 C24 1.33(2) . ? C23 Hf2 2.512(14) . ? C23 H23 0.95 . ? C24 C25 1.44(2) . ? C24 Hf2 2.517(14) . ? C24 H24 0.95 . ? C25 C26 1.43(2) . ? C25 Hf2 2.468(15) . ? C25 H25 0.95 . ? C26 Hf2 2.512(14) . ? C26 H26 0.95 . ? C27 C28 1.41(2) . ? C27 C31 1.41(2) . ? C27 Hf2 2.482(14) . ? C27 H27 0.95 . ? C28 C29 1.39(2) . ? C28 Hf2 2.483(14) . ? C28 H28 0.95 . ? C29 C30 1.39(2) . ? C29 Hf2 2.510(15) . ? C29 H29 0.95 . ? C30 C31 1.42(2) . ? C30 Hf2 2.551(14) . ? C30 H30 0.95 . ? C31 Hf2 2.524(15) . ? C31 H31 0.95 . ? C32 Si2 1.868(15) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 Si2 1.875(14) . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 Si2 1.899(14) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 N3 1.423(18) . ? C35 C36 1.503(19) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 N3 1.505(17) . ? C37 C38 1.52(2) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 C40 1.44(2) . ? C39 N4 1.511(19) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 N4 1.468(18) . ? C41 C42 1.481(19) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? N1 P2 1.725(12) . ? N2 P2 1.671(12) . ? N3 P4 1.710(11) . ? N4 P4 1.698(12) . ? Si1 P1 2.266(5) . ? Si2 P3 2.273(5) . ? P1 P2 2.240(5) . ? P1 Hf1 2.648(4) . ? P3 P4 2.236(5) . ? P3 Hf2 2.637(4) . ? Cl1 Hf1 2.429(3) . ? Cl2 Hf2 2.412(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 108.7(12) . . ? C2 C1 Hf1 74.9(8) . . ? C5 C1 Hf1 72.0(8) . . ? C2 C1 H1 125.6 . . ? C5 C1 H1 125.6 . . ? Hf1 C1 H1 119.2 . . ? C1 C2 C3 106.9(12) . . ? C1 C2 Hf1 72.9(8) . . ? C3 C2 Hf1 72.0(7) . . ? C1 C2 H2 126.6 . . ? C3 C2 H2 126.6 . . ? Hf1 C2 H2 120.4 . . ? C2 C3 C4 108.5(12) . . ? C2 C3 Hf1 75.1(7) . . ? C4 C3 Hf1 73.4(8) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Hf1 C3 H3 117.7 . . ? C5 C4 C3 107.1(13) . . ? C5 C4 Hf1 72.8(8) . . ? C3 C4 Hf1 73.3(8) . . ? C5 C4 H4 126.4 . . ? C3 C4 H4 126.4 . . ? Hf1 C4 H4 119.4 . . ? C4 C5 C1 108.7(14) . . ? C4 C5 Hf1 74.7(9) . . ? C1 C5 Hf1 74.8(8) . . ? C4 C5 H5 125.7 . . ? C1 C5 H5 125.7 . . ? Hf1 C5 H5 116.8 . . ? C7 C6 C10 108.0(13) . . ? C7 C6 Hf1 73.9(8) . . ? C10 C6 Hf1 74.9(7) . . ? C7 C6 H6 126 . . ? C10 C6 H6 126 . . ? Hf1 C6 H6 117.2 . . ? C8 C7 C6 107.6(14) . . ? C8 C7 Hf1 74.0(8) . . ? C6 C7 Hf1 72.3(8) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Hf1 C7 H7 119.4 . . ? C7 C8 C9 107.1(14) . . ? C7 C8 Hf1 73.0(8) . . ? C9 C8 Hf1 74.0(8) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? Hf1 C8 H8 118.6 . . ? C10 C9 C8 109.9(14) . . ? C10 C9 Hf1 73.9(8) . . ? C8 C9 Hf1 72.5(8) . . ? C10 C9 H9 125.1 . . ? C8 C9 H9 125.1 . . ? Hf1 C9 H9 120.2 . . ? C9 C10 C6 107.4(13) . . ? C9 C10 Hf1 74.3(8) . . ? C6 C10 Hf1 71.3(7) . . ? C9 C10 H10 126.3 . . ? C6 C10 H10 126.3 . . ? Hf1 C10 H10 120 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 113.6(13) . . ? N1 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N1 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 112.0(13) . . ? N1 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N1 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N2 114.5(12) . . ? C19 C18 H18A 108.6 . . ? N2 C18 H18A 108.6 . . ? C19 C18 H18B 108.6 . . ? N2 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C21 113.9(12) . . ? N2 C20 H20A 108.8 . . ? C21 C20 H20A 108.8 . . ? N2 C20 H20B 108.8 . . ? C21 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C26 C22 C23 104.6(13) . . ? C26 C22 Hf2 74.4(9) . . ? C23 C22 Hf2 73.0(8) . . ? C26 C22 H22 127.7 . . ? C23 C22 H22 127.7 . . ? Hf2 C22 H22 117.3 . . ? C24 C23 C22 110.7(12) . . ? C24 C23 Hf2 74.9(8) . . ? C22 C23 Hf2 72.9(8) . . ? C24 C23 H23 124.6 . . ? C22 C23 H23 124.6 . . ? Hf2 C23 H23 119.2 . . ? C23 C24 C25 107.8(13) . . ? C23 C24 Hf2 74.5(9) . . ? C25 C24 Hf2 71.4(8) . . ? C23 C24 H24 126.1 . . ? C25 C24 H24 126.1 . . ? Hf2 C24 H24 119.9 . . ? C26 C25 C24 105.9(13) . . ? C26 C25 Hf2 75.0(8) . . ? C24 C25 Hf2 75.1(8) . . ? C26 C25 H25 127 . . ? C24 C25 H25 127 . . ? Hf2 C25 H25 115.3 . . ? C22 C26 C25 110.8(14) . . ? C22 C26 Hf2 74.3(9) . . ? C25 C26 Hf2 71.7(9) . . ? C22 C26 H26 124.6 . . ? C25 C26 H26 124.6 . . ? Hf2 C26 H26 121 . . ? C28 C27 C31 108.3(14) . . ? C28 C27 Hf2 73.6(8) . . ? C31 C27 Hf2 75.3(9) . . ? C28 C27 H27 125.9 . . ? C31 C27 H27 125.9 . . ? Hf2 C27 H27 117.3 . . ? C29 C28 C27 106.8(14) . . ? C29 C28 Hf2 74.9(8) . . ? C27 C28 Hf2 73.5(9) . . ? C29 C28 H28 126.6 . . ? C27 C28 H28 126.6 . . ? Hf2 C28 H28 117.2 . . ? C28 C29 C30 110.6(13) . . ? C28 C29 Hf2 72.7(8) . . ? C30 C29 Hf2 75.6(8) . . ? C28 C29 H29 124.7 . . ? C30 C29 H29 124.7 . . ? Hf2 C29 H29 118.6 . . ? C29 C30 C31 106.2(14) . . ? C29 C30 Hf2 72.4(9) . . ? C31 C30 Hf2 72.7(8) . . ? C29 C30 H30 126.9 . . ? C31 C30 H30 126.9 . . ? Hf2 C30 H30 120 . . ? C27 C31 C30 108.2(14) . . ? C27 C31 Hf2 72.0(8) . . ? C30 C31 Hf2 74.8(8) . . ? C27 C31 H31 125.9 . . ? C30 C31 H31 125.9 . . ? Hf2 C31 H31 119.1 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 C36 120.1(12) . . ? N3 C35 H35A 107.3 . . ? C36 C35 H35A 107.3 . . ? N3 C35 H35B 107.3 . . ? C36 C35 H35B 107.3 . . ? H35A C35 H35B 106.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 C38 111.3(11) . . ? N3 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? N3 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 N4 118.5(15) . . ? C40 C39 H39A 107.7 . . ? N4 C39 H39A 107.7 . . ? C40 C39 H39B 107.7 . . ? N4 C39 H39B 107.7 . . ? H39A C39 H39B 107.1 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 C42 116.6(12) . . ? N4 C41 H41A 108.1 . . ? C42 C41 H41A 108.1 . . ? N4 C41 H41B 108.1 . . ? C42 C41 H41B 108.1 . . ? H41A C41 H41B 107.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C16 N1 C14 115.1(12) . . ? C16 N1 P2 127.0(10) . . ? C14 N1 P2 114.8(10) . . ? C20 N2 C18 111.8(11) . . ? C20 N2 P2 117.7(10) . . ? C18 N2 P2 122.4(9) . . ? C35 N3 C37 112.5(11) . . ? C35 N3 P4 120.2(10) . . ? C37 N3 P4 123.5(9) . . ? C41 N4 C39 114.6(12) . . ? C41 N4 P4 125.6(9) . . ? C39 N4 P4 118.9(10) . . ? C13 Si1 C11 103.5(7) . . ? C13 Si1 C12 108.2(7) . . ? C11 Si1 C12 109.6(7) . . ? C13 Si1 P1 115.9(5) . . ? C11 Si1 P1 112.5(5) . . ? C12 Si1 P1 107.0(5) . . ? C32 Si2 C33 110.2(7) . . ? C32 Si2 C34 105.7(7) . . ? C33 Si2 C34 105.6(6) . . ? C32 Si2 P3 108.7(5) . . ? C33 Si2 P3 114.7(5) . . ? C34 Si2 P3 111.7(5) . . ? P2 P1 Si1 99.16(19) . . ? P2 P1 Hf1 112.83(17) . . ? Si1 P1 Hf1 110.52(17) . . ? N2 P2 N1 112.4(6) . . ? N2 P2 P1 102.3(4) . . ? N1 P2 P1 98.8(4) . . ? P4 P3 Si2 98.8(2) . . ? P4 P3 Hf2 115.35(18) . . ? Si2 P3 Hf2 115.85(17) . . ? N4 P4 N3 111.9(6) . . ? N4 P4 P3 104.0(4) . . ? N3 P4 P3 99.3(4) . . ? Cl1 Hf1 C6 134.8(4) . . ? Cl1 Hf1 C7 117.0(4) . . ? C6 Hf1 C7 33.8(5) . . ? Cl1 Hf1 C5 95.7(3) . . ? C6 Hf1 C5 97.6(5) . . ? C7 Hf1 C5 131.3(5) . . ? Cl1 Hf1 C8 85.1(3) . . ? C6 Hf1 C8 55.3(5) . . ? C7 Hf1 C8 33.0(5) . . ? C5 Hf1 C8 133.9(5) . . ? Cl1 Hf1 C10 107.6(3) . . ? C6 Hf1 C10 33.8(5) . . ? C7 Hf1 C10 55.7(5) . . ? C5 Hf1 C10 81.5(5) . . ? C8 Hf1 C10 55.0(5) . . ? Cl1 Hf1 C9 80.8(4) . . ? C6 Hf1 C9 54.4(5) . . ? C7 Hf1 C9 54.8(5) . . ? C5 Hf1 C9 100.9(5) . . ? C8 Hf1 C9 33.6(5) . . ? C10 Hf1 C9 31.8(5) . . ? Cl1 Hf1 C3 130.1(3) . . ? C6 Hf1 C3 91.8(5) . . ? C7 Hf1 C3 112.3(5) . . ? C5 Hf1 C3 54.4(5) . . ? C8 Hf1 C3 144.8(5) . . ? C10 Hf1 C3 105.8(5) . . ? C9 Hf1 C3 137.5(5) . . ? Cl1 Hf1 C4 128.0(4) . . ? C6 Hf1 C4 76.2(5) . . ? C7 Hf1 C4 107.8(5) . . ? C5 Hf1 C4 32.5(5) . . ? C8 Hf1 C4 129.2(5) . . ? C10 Hf1 C4 76.7(5) . . ? C9 Hf1 C4 106.7(5) . . ? C3 Hf1 C4 33.3(5) . . ? Cl1 Hf1 C1 78.9(3) . . ? C6 Hf1 C1 129.1(5) . . ? C7 Hf1 C1 162.1(5) . . ? C5 Hf1 C1 33.2(5) . . ? C8 Hf1 C1 156.3(5) . . ? C10 Hf1 C1 113.7(5) . . ? C9 Hf1 C1 125.3(5) . . ? C3 Hf1 C1 53.9(4) . . ? C4 Hf1 C1 54.3(5) . . ? Cl1 Hf1 C2 97.9(3) . . ? C6 Hf1 C2 124.7(5) . . ? C7 Hf1 C2 141.2(5) . . ? C5 Hf1 C2 54.5(4) . . ? C8 Hf1 C2 171.0(4) . . ? C10 Hf1 C2 131.0(5) . . ? C9 Hf1 C2 155.2(5) . . ? C3 Hf1 C2 32.9(5) . . ? C4 Hf1 C2 54.8(5) . . ? C1 Hf1 C2 32.2(4) . . ? Cl1 Hf1 P1 95.91(11) . . ? C6 Hf1 P1 106.6(4) . . ? C7 Hf1 P1 82.5(4) . . ? C5 Hf1 P1 131.5(3) . . ? C8 Hf1 P1 94.0(3) . . ? C10 Hf1 P1 137.7(3) . . ? C9 Hf1 P1 127.4(4) . . ? C3 Hf1 P1 83.0(3) . . ? C4 Hf1 P1 115.4(3) . . ? C1 Hf1 P1 104.9(3) . . ? C2 Hf1 P1 77.3(3) . . ? Cl2 Hf2 C25 135.1(4) . . ? Cl2 Hf2 C27 104.8(4) . . ? C25 Hf2 C27 95.0(5) . . ? Cl2 Hf2 C28 132.7(4) . . ? C25 Hf2 C28 83.0(5) . . ? C27 Hf2 C28 32.9(5) . . ? Cl2 Hf2 C29 118.0(3) . . ? C25 Hf2 C29 106.3(5) . . ? C27 Hf2 C29 53.5(5) . . ? C28 Hf2 C29 32.4(5) . . ? Cl2 Hf2 C22 81.4(4) . . ? C25 Hf2 C22 54.8(5) . . ? C27 Hf2 C22 125.7(5) . . ? C28 Hf2 C22 134.3(5) . . ? C29 Hf2 C22 160.6(5) . . ? Cl2 Hf2 C26 109.4(4) . . ? C25 Hf2 C26 33.3(5) . . ? C27 Hf2 C26 127.0(5) . . ? C28 Hf2 C26 115.0(5) . . ? C29 Hf2 C26 130.4(5) . . ? C22 Hf2 C26 31.3(5) . . ? Cl2 Hf2 C23 85.7(3) . . ? C25 Hf2 C23 53.3(5) . . ? C27 Hf2 C23 91.8(5) . . ? C28 Hf2 C23 108.4(5) . . ? C29 Hf2 C23 140.7(5) . . ? C22 Hf2 C23 34.1(5) . . ? C26 Hf2 C23 52.9(5) . . ? Cl2 Hf2 C24 114.6(3) . . ? C25 Hf2 C24 33.5(5) . . ? C27 Hf2 C24 75.3(5) . . ? C28 Hf2 C24 80.9(5) . . ? C29 Hf2 C24 112.8(5) . . ? C22 Hf2 C24 54.6(5) . . ? C26 Hf2 C24 54.1(5) . . ? C23 Hf2 C24 30.7(5) . . ? Cl2 Hf2 C31 78.4(4) . . ? C25 Hf2 C31 127.6(5) . . ? C27 Hf2 C31 32.7(5) . . ? C28 Hf2 C31 54.2(5) . . ? C29 Hf2 C31 53.1(5) . . ? C22 Hf2 C31 139.2(5) . . ? C26 Hf2 C31 157.7(5) . . ? C23 Hf2 C31 108.9(5) . . ? C24 Hf2 C31 103.6(5) . . ? Cl2 Hf2 C30 86.3(4) . . ? C25 Hf2 C30 136.4(5) . . ? C27 Hf2 C30 54.1(5) . . ? C28 Hf2 C30 54.2(5) . . ? C29 Hf2 C30 32.0(4) . . ? C22 Hf2 C30 167.1(5) . . ? C26 Hf2 C30 161.4(5) . . ? C23 Hf2 C30 141.3(5) . . ? C24 Hf2 C30 129.1(5) . . ? C31 Hf2 C30 32.5(5) . . ? Cl2 Hf2 P3 97.14(12) . . ? C25 Hf2 P3 98.9(3) . . ? C27 Hf2 P3 131.7(4) . . ? C28 Hf2 P3 103.7(4) . . ? C29 Hf2 P3 78.2(3) . . ? C22 Hf2 P3 99.6(3) . . ? C26 Hf2 P3 82.6(4) . . ? C23 Hf2 P3 132.9(3) . . ? C24 Hf2 P3 132.0(3) . . ? C31 Hf2 P3 117.8(4) . . ? C30 Hf2 P3 85.7(4) . . ? # END of CIF _chemical_name_common ; ((Bis- diethylaminophosphanyl)(trimethylsilyl)phosphide)(chlorido) (bis- cyclopentadienylo) hafnium(IV) ;